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Method for preparing fluorinated graphene through microwave hydrothermal method

A technology of fluorinated graphene and microwave hydrothermal method, applied in graphene, nano-carbon and other directions, can solve the problems of complex equipment required for the reaction, harsh reaction conditions, and high cost of raw materials, so that it is easy to popularize and use, and has few influencing factors. , the effect of reducing energy consumption

Inactive Publication Date: 2013-09-11
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] In order to avoid the deficiencies of the prior art, the present invention proposes a method for preparing fluorinated graphene by microwave hydrothermal method, which solves the high cost of raw materials used in the reaction and the equipment required for the reaction in the existing preparation method of fluorinated graphene. Complexity, harsh reaction conditions, high energy consumption, low yield and other technical problems, a method for preparing fluorinated graphene by microwave hydrothermal method with simple preparation process, high efficiency, low cost and high yield was proposed

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  • Method for preparing fluorinated graphene through microwave hydrothermal method
  • Method for preparing fluorinated graphene through microwave hydrothermal method
  • Method for preparing fluorinated graphene through microwave hydrothermal method

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Embodiment 1

[0025] (1) Preparation of aqueous dispersion of graphene oxide: place the flask in an ice-water bath, pour an appropriate amount of concentrated sulfuric acid; mix 3g flake graphite powder, 1.5g NaNO 3 Pour into the flask, stir evenly, and then cool for 3h, so that the temperature of the system is 0°C; add 9g KMnO to the mixed solution 4 , stir evenly, and keep the system temperature below 20°C during this period; move the flask into an oil bath, keep the temperature at 35°C for 2 hours, add deionized water, and after 10 minutes, add diluted hydrogen peroxide to obtain a bright yellow solution; filter the reactants, and use Repeated washing with 10% hydrochloric acid and distilled water, suction filtration, dialyzing the obtained viscous solid until the pH value is close to neutral; drying and grinding the obtained solid to obtain graphite oxide; weigh 100mg of graphite oxide, measure 50mL of distilled water, and pour it into a beaker , using an ultrasonic cleaner (40KHz, 100W...

Embodiment 2

[0031] (1) Preparation of aqueous dispersion of graphene oxide: place the flask in an ice-water bath, pour an appropriate amount of concentrated sulfuric acid; mix 3g flake graphite powder, 1.5g NaNO 3 Pour into the flask, stir evenly, and then cool for 3h, so that the temperature of the system is 0°C; add 9g KMnO to the mixed solution 4 , stir evenly, and keep the system temperature below 20°C during this period; move the flask into an oil bath, keep the temperature at 35°C for 2 hours, add deionized water, and after 10 minutes, add diluted hydrogen peroxide to obtain a bright yellow solution; filter the reactants, and use Repeated washing with 10% hydrochloric acid and distilled water, suction filtration, dialyzing the obtained viscous solid until the pH value is close to neutral; drying and grinding the obtained solid to obtain graphite oxide; weigh 60mg of graphite oxide, measure 60mL of distilled water, and pour it into a beaker , using an ultrasonic cleaner (40KHz, 100W)...

Embodiment 3

[0037] (1) Preparation of aqueous dispersion of graphene oxide: place the flask in an ice-water bath, pour an appropriate amount of concentrated sulfuric acid; mix 3g flake graphite powder, 1.5g NaNO 3 Pour into the flask, stir evenly, and then cool for 3h, so that the temperature of the system is 0°C; add 9g KMnO to the mixed solution 4 , stir evenly, and keep the system temperature below 20°C during this period; move the flask into an oil bath, keep the temperature at 35°C for 2 hours, add deionized water, and after 10 minutes, add diluted hydrogen peroxide to obtain a bright yellow solution; filter the reactants, and use Repeated washing with 10% hydrochloric acid and distilled water, suction filtration, dialyzing the obtained viscous solid until the pH value is close to neutral; drying and grinding the obtained solid to obtain graphite oxide; weigh 80mg of graphite oxide, measure 60mL of distilled water, and pour it into a beaker , using an ultrasonic cleaner (40KHz, 100W)...

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Abstract

The invention provides a method for preparing fluorinated graphene through a microwave hydrothermal method. The fluorinated graphene is prepared by employing the microwave hydrothermal method and is rapidly heated by utilizing the change of the electric field and magnetic field in the space, the low-temperature (150-200 DEG C) temperature is realized, the reaction time (30-60 minutes) is greatly shortened, the energy consumption is reduced, and the preparation efficiency is improved. The adopted preparation method does not have temperature gradient in the reaction process, a hysteresis effect is avoided, and the reaction process is easy to control and fewer in influence factors; and the prepared fluorinated graphene is uniform in fluorine doping and high in experimental repeatability. The process conditions such as raw material ratio, reaction temperature and reaction time are adjusted, and the fluorinated graphene of different fluorine contents can be prepared. The prepared fluorinated graphene is high in yield, and the yield is up to 90-95 percent. The preparation method is easily popularized and applied.

Description

technical field [0001] The invention belongs to the field of material synthesis chemistry, and in particular relates to a method for preparing fluorinated graphene by a microwave hydrothermal method. Background technique [0002] Graphene is a two-dimensional material with carbon atoms arranged in a hexagonal grid. Since 2004, the Geim group of the University of Manchester in the United Kingdom has prepared and observed the existence of single-layer graphene by tape stripping method. Graphene has become a hot spot in nanomaterial research because of its excellent optical, electrical, mechanical, thermal, and magnetic properties. The fluorination of graphene is an effective method to tune the electronic structure and physicochemical properties of graphene materials. Studies have shown that with different degrees of fluorination, the band gap of fluorinated graphene can be adjusted from 0eV to 3eV, and the highest band gap can reach 3.1eV. Fluorinated graphene has potential ...

Claims

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Application Information

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IPC IPC(8): C01B31/00C01B32/184
Inventor 李贺军罗慧娟付前刚沈庆凉
Owner NORTHWESTERN POLYTECHNICAL UNIV
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